Solution thermal method was used to synthesize CuInSe2 powders from metal chlorides and SeO2 at 160~200°C. The phases of product samples were analyzed by x-ray diffraction (XRD), the size and morphology of the products were observed by JSM6380LA scanning electron microscope (SEM). The aim is to explore the best technology to obtain the pure CuInSe2 powders. Experimental results show that, CuInSe2 phase can be formed with metal chlorides by reacting for 20 h at 160°C, 180°C and 200°C and has XRD peaks corresponding to (112), (204) and (312) crystal planes, respectively. It consists of irregular spherical grains with about 0.2~0.5 μm in diameter, which agglomerate larger particles with average particle size about 1~3 μm. CuInSe2 phase was formed more easily at the temperature higher than 180°C and shows better crystallinity.